CN105295434B - Method for combined extraction of haematochrome and pectin from pitaya peel - Google Patents
Method for combined extraction of haematochrome and pectin from pitaya peel Download PDFInfo
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- CN105295434B CN105295434B CN201510788412.0A CN201510788412A CN105295434B CN 105295434 B CN105295434 B CN 105295434B CN 201510788412 A CN201510788412 A CN 201510788412A CN 105295434 B CN105295434 B CN 105295434B
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- haematochrome
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Abstract
The invention discloses a method for combined extraction of haematochrome and pectin from pitaya peel. The method comprises the following specific steps: firstly chopping pitaya peel, blanching, drying, crushing, extracting by adding ethanol, filtering, and respectively collecting a filtrate and filter residue; carrying out extraction purification on the filtrate respectively by using a polyethylene glycol/ammonium sulfate aqueous two-phase system and trichloromethane so as to obtain a viscous pasty pitaya haematochrome; washing the filter residue with water to remove alcohol and carrying out heat insulation and acidolysis, processing by adding cation exchange resin and filtering, concentrating a filtrate, precipitating with ethanol, centrifuging, drying and crushing so as to obtain flaxen pectin powder. The method of the invention has advantages of simple equipment and low cost. In addition, high-purity haematochrome and high-ester pectin can be simultaneously extracted from pitaya peel. Thus, resource wasting caused by single extraction is avoided, and comprehensive utilization rate of pitaya can be remarkably raised.
Description
Technical field
The invention belongs to agricultural byproducts comprehensive utilization deep process technology field, and in particular to one kind joins from dragon fruit pericarp
Close the method for extracting haematochrome and pectin.
Background technology
Dragon fruit also known as Pitaya fruit, Hylocereus undatus etc., are a kind of tropical fruit (tree)s of high nutritive value, with aid digestion, drop blood
The plurality of health care functions such as pressure, hypoglycemic, anti-oxidant, it is deep to be liked by consumer.China's dragon fruit cultivated area in 2013 is up to 100,000
Many mu, there is the trend for constantly expanding at present.
Dragon fruit pericarp accounts for a quarter of fruit weight, and it is rich in the native chemical composition such as haematochrome and pectin.But in food
During product are processed with daily consumption, dragon fruit pericarp Jing is often taken as waste material and directly abandons, and causes the huge wasting of resources.
Haematochrome in dragon fruit pericarp is mainly Betacyanins and its glycoside, and it has anti-oxidant, removing free radical, raising well
The physiological function such as immunity and anticancer, can be used as natural food colour or food additives with health role；And pectin is
The main component of soluble dietary fiber in human body seven major nutrient, and it also has good gelatine and emulsification,
It is widely used in food, medicine and cosmetics industry.
Some are had at present using the technology research that dragon fruit pericarp is raw material extraction haematochrome and pectin.Such as patent
CN 1631987A disclose a kind of method that water-soluble red colouring matter is extracted from dragon fruit pulp, pericarp；Patent CN
103497534A discloses one kind and utilizes supercritical CO2The method of fluid extraction dragon fruit pericarp pigment；Patent CN
104212196A discloses a kind of preparation method of haematochrome in dragon fruit pericarp；Yuan Yafang etc.（" red meat dragon fruit pericarp pigment
Separate, purifying and HPLC-MS are analyzed ", University Of Agriculture and Forestry In Fujian's journal (natural science edition), 2013,42 (6):589-592）Report
Separation, the purifying research of red meat dragon fruit pericarp pigment；King's mark poem etc.（" the extraction of dragon fruit pericarp pigment and its anti-oxidant
The research of activity ", food industry science and technology, 2013 (43) 5:234-238）Report extraction and its antioxygen of dragon fruit pericarp pigment
Change the research of activity；Wang Xue etc. (" extraction and its structural research of pectin in pitaya peel ", Food Additives Used in China, 2015,3:
102-106) report the extraction and its structural research of pectin in pitaya peel；(" red meat dragon fruit pericarp pectin is carried Chen Jingjing etc.
The optimizing research of taking technique condition ", southern china fruit tree, 2014,43 (3)：96-98) report red meat dragon fruit pericarp pectin
The optimizing research of extracting factor.These patents and document are confined to the separation and Extraction of single component in dragon fruit pericarp,
Raw material cannot be fully used, and in the extraction process of these single components, and some only obtain haematochrome, pectin
Crude product, containing impurity such as substantial amounts of carbohydrates in these crude products, its quality does not reach industrial requirements；Some technology utilizations are super to be faced
Boundary CO2Fluid or high performance liquid chromatograph are isolated and purified to haematochrome, although purity reaches requirement, but it is high to there is equipment
The deficiency such as expensive, production cost is high；Employing macroporous absorbent resin also carries out absorption and purification, though can be by substantial amounts of impurity
Separate remove, but resin absorption and wash-out the cycle it is long, increased the complexity of operation.
The content of the invention
The purpose of the present invention is for the deficiencies in the prior art, there is provided one kind is from combined extracting haematochrome in dragon fruit pericarp
With the method for pectin, its device therefor is simple and convenient to operate, extraction cost is low, product purity is high, is remarkably improved dragon fruit fruit
The comprehensive utilization ratio of skin resource.
For achieving the above object, the present invention is adopted the following technical scheme that：
The method of combined extracting haematochrome and pectin, specifically includes following steps in a kind of pericarp from dragon fruit：
1）Inactivate pectase the chopping of fresh dragon fruit pericarp, 5 ~ 8min of boiling water boiling, clear water rinsing post-drying, crushing；
2）By step poly- 1）Gained powder adds 5 ~ 10 times of its volume, mass concentration is 70% ethanol, extraction 1 under room temperature ~
2h, filters, and filtrate and filter residue are collected respectively；
3）By step poly- 2）Gained filtrate is concentrated in vacuo to after doing at 50-55 DEG C, with polyethylene glycol/ammonium sulfate aqueous two-phase body
System carries out abstraction purification；Upper strata dark red solution is the polyglycol solution containing haematochrome, lower floor's light red solution be containing
The ammonium sulfate of the impurity such as carbohydrate；
4）Take step poly- 3）Upper solution, adds isopyknic chloroform extraction, haematochrome to enter the aqueous phase solution on upper strata,
Polyethylene glycol enters the organic phase solution of lower floor, separates dragon fruit haematochrome and polyethylene glycol, collects upper strata aqueous phase solution；
5）By step poly- 4）Gained aqueous phase solution is concentrated in vacuo at 50 ~ 55 DEG C, obtains the dragon fruit haematochrome of sticky paste；
6）By step poly- 2）Gained filter residue tap water rinse, remove residual ethanol, add 5 ~ 10 times of filter residue volume go from
The oxalic acid of sub- water and filter residue weight 1 ~ 3%, is 3.0 ~ 3.6 with sodium hydrate regulator solution pH value, is then heated to 60 ~ 80 DEG C, is delayed
Slow agitation 60min, filters, and collects filtrate；
7）By step poly- 6）Gained filtrate adds ion exchange resin, and 30 ~ 60min is slowly stirred under room temperature, filters, and collects filter
Liquid；
8）By step poly- 7）Gained filter vacuum is concentrated into the 1/4 ~ 1/5 of original volume, is subsequently adding the anhydrous second of 1-2 times of volume
Alcohol, Jing centrifugations, precipitation, drying, crushing, obtains final product flaxen jelly powder.
Walk poly- 3）Middle polyethylene glycol/ammonium sulfate double-aqueous phase system abstraction purification is specifically by polyglycol solution and ammonium sulfate
Solution is added in filtrate, and Jing after 20 ~ 30min of magnetic agitation, it is 5.0 ~ 5.5 to adjust solution ph, and 6 ~ 12h is stood under room temperature,
It is layered it；
The mass concentration of polyethylene glycol is 15 ~ 25% in the polyethylene glycol/ammonium sulfate double-aqueous phase system, the matter of ammonium sulfate
Amount concentration is 10 ~ 15%；The molecular weight optional 2000,4000 and 6000, preferably 6000 of polyethylene glycol used.
Step 7）Described in ion exchange resin be storng-acid cation exchange resin, its consumption for filter residue weight 1 ~
2%。
Step 2）With step 8）In ethanol used it is recovered after can be recycled.
Compared with prior art, the present invention has following remarkable advantage：
(1) present invention achieves dragon fruit pericarp haematochrome, the combined extracting of two kinds of materials of pectin, and yield and purity with
It is existing it is single extract a kind of material quite, but avoid it is single extract the brought wasting of resources, substantially increase fiery fruit dragon
Comprehensive utilization ratio.
(2) when extraction purification is carried out to dragon fruit pericarp haematochrome, ethanol solution of the present invention first with low concentration
Extracted, obtained haematochrome crude extract, then recycled polyethylene glycol/ammonium sulfate double-aqueous phase system by the redness in crude extract
Element is separated with the impurity such as carbohydrate.Because polyethylene glycol/ammonium sulfate aqueous two phase extraction technique can be carried out in a mild condition, from
And the stability of haematochrome is farthest ensure that, and its separative efficiency is high, and the time is short, without the need for large-scale and complicated device, behaviour
Make easy.
(3) due to being rich in Ca in dragon fruit pericarp2+、Mg2+Plasma, has sealing process to pectin, can affect protopectin to
Water soluble pectin is converted, therefore its recovery rate of the acidity extraction pectin of routine is low, gained pectin is of poor quality.The present invention is replaced using oxalic acid
Inorganic acid used in generation conventional acid hydrolyzation（Hydrochloric acid, sulfuric acid, phosphoric acid etc.）Acidolysis is carried out, is had using oxalate denominationby very strong
Metal-chelating act on, can well by pericarp membrane wall with Ca2+、Mg2+The water-insoluble pectin extraction that chelating is formed goes out
Come, while adding the remaining cation of ion exchange resin absorption in pectin solution, the recovery rate and quality of pectin can be improved.
Description of the drawings
Fig. 1 is the UV-Vis spectra figure of the dragon fruit pericarp haematochrome solution of the preparation of the present invention.
Fig. 2 is the UV-Vis spectra figure of the dragon fruit pericarp haematochrome solution after single extraction purification.
Specific embodiment
In order that content of the present invention easily facilitates understanding, with reference to specific embodiment to of the present invention
Technical scheme is described further, but the present invention is not limited only to this.
Combined extracting haematochrome and pectin in embodiment dragon fruit pericarp
The method of combined extracting haematochrome and pectin, specifically includes following steps in a kind of pericarp from dragon fruit：
1）The fresh dragon fruit pericarp that 400g removes green scale is cut into into the fritter that size is 3-4mm, boiling water boiling 5min,
Inactivate pectase, clear water rinsing is pressed dry afterwards for several times, and in 60 DEG C of baking ovens 12h is dried, and is subsequently cooled to room temperature, is crushed with cooking machine
Into powder；The gained ethanol that powder adds 5 times of its volume, mass concentration is 70%, extracts 2h under room temperature, filter, and filter is collected respectively
Liquid and filter residue；
2）By step poly- 1）Gained filtrate is concentrated in vacuo to after doing at 50 DEG C, adds PEG6000 and ammonium sulfate, makes institute
The mass concentration for obtaining polyethylene glycol in polyethylene glycol/ammonium sulfate double-aqueous phase system is 15%, and the mass concentration of ammonium sulfate is 10%, then
Jing after magnetic agitation 30min, it is 5.0 to adjust solution ph, stands 6h under room temperature so as to be layered, and upper strata dark red solution is to contain
There is the polyglycol solution of haematochrome, lower floor's light red solution is the ammonium sulfate containing impurity such as carbohydrates；Take the poly- upper strata of step
Solution, after adding isopyknic chloroform to be well mixed, 3000rpm centrifugation 10min make haematochrome mix into the water on upper strata
Liquid, polyethylene glycol enters the organic phase solution of lower floor, collects upper strata aqueous phase solution；The poly- gained aqueous phase solution of step is true at 50 DEG C
Sky concentration, obtains the dragon fruit water-soluble natural haematochrome 5.68g of sticky paste, and yield is 1.42%；
3）By step poly- 1）Gained filter residue tap water rinse, removes residual ethanol, adds 5 times of deionized waters of filter residue volume
It is 3.0 with sodium hydrate regulator solution pH value with the oxalic acid of filter residue weight 3%, is then heated to 60 DEG C, slowly stirs 60min,
Filter after 3000rpm centrifugation 10min, collect filtrate；By the poly- gained filtrate of step add the 721 type highly acids sun of filter residue weight 1% from
60min is slowly stirred under sub-exchange resin, room temperature, is filtered, collect filtrate；Gained filter vacuum is concentrated into into the 1/4 of original volume,
The absolute ethyl alcohol of 2 times of volumes is subsequently adding, room temperature is placed 6000rpm centrifugations 10min after 2h, obtains pectin precipitation, then will fruit
Glue is deposited in 65 DEG C of vacuum desiccators and dries, and takes out levigate, obtains flaxen jelly powder 1.93g, Jing conversions, and its yield is
4.82g/kg（Fresh weight）, Jing FCC titration measurings, the esterification degree of gained pectin is 64.6, is high-ester pectin.
Gained dragon fruit haematochrome 1.0g is taken, in being dissolved in 100mL pure water, its suction is scanned in the range of the nm of wavelength 400 ~ 660
Luminosity, as a result as shown in Figure 1.Gained dragon fruit haematochrome has obvious absworption peak in visible region, and its maximum absorption wave is a length of
538nm, illustrates that its main component is beet glycoside pigment.The absorbance that haematochrome solution is determined under 538nm is 0.830,
According to colour value computing formula, the colour value of dragon fruit haematochrome is conversed538nm =83.0。
The single extraction of haematochrome in the dragon fruit pericarp of comparative example 1
1）The fresh dragon fruit pericarp that 400g removes green scale is cut into into the fritter that size is 3-4mm, boiling water boiling 5min,
Inactivate pectase, clear water rinsing is pressed dry afterwards for several times, and in 60 DEG C of baking ovens 12h is dried, and is subsequently cooled to room temperature, is crushed with cooking machine
Into powder；The gained ethanol that powder adds 5 times of its volume, mass concentration is 70%, extracts 2h under room temperature, filter, and collects filtrate；
2）Gained filtrate is adsorbed by D101 macroreticular resins, obtains being adsorbed with the macropore tree of dragon fruit haematochrome
Fat, then elutes to macroreticular resin, collects eluent, concentrated in vacuo under the conditions of temperature 50-55 DEG C with Rotary Evaporators,
The dragon fruit water-soluble natural haematochrome 6.42g of sticky paste is obtained, haematochrome yield is 1.60%.
Get fire imperial arnotto pigment 1.0g, in being dissolved in 100mL pure water, in the range of the nm of wavelength 400 ~ 660 its extinction is scanned
Degree, as a result as shown in Figure 2.Gained dragon fruit haematochrome has two obvious absworption peaks in visible region 480nm and 538nm, this
Two wavelength are respectively the maximum absorption wavelength of betaxanthin and beet red glycosides, illustrate dragon fruit haematochrome crude extract Jing macropore trees
Fat after purification, still with the presence of part betaxanthin.The absorbance that haematochrome solution is measured in 538nm is 0.698, according to colour value
Computing formula, converses the colour value of dragon fruit haematochrome538nm =69.8。
The single extraction of pectin in the dragon fruit pericarp of comparative example 2
1）The fresh dragon fruit pericarp that 400g removes green scale is cut into into the fritter that size is 3-4mm, boiling water boiling 5min,
Inactivate pectase, clear water rinsing is pressed dry afterwards for several times, and in 60 DEG C of baking ovens 12h is dried, and is subsequently cooled to room temperature, is crushed with cooking machine
Into powder；Gained powder adds the deionized water of its 5 times of volumes, with salt acid for adjusting pH to 1.5 ~ 1.6, at 80 DEG C acidolysis is stirred
Filter after 60min, 3000rpm centrifugation 10min, collect filtrate；Gained filtrate rotary evaporation is concentrated into the 1/4 of original volume, then
The absolute ethyl alcohol of 2 times of volumes, room temperature is added to place 6000rpm centrifugations 10min after 2h, obtain pectin precipitation；Gained pectin is sunk
Form sediment and dried in 65 DEG C of vacuum desiccators, take out levigate, obtain jelly powder 1.58g, after conversion, its yield is 3.96g/kg（It is fresh
Weight）, Jing FCC titration measurings, the esterification degree of gained pectin is 31.4, belongs to low-ester pectin.
Visible with the comparison of comparative example 1 by embodiment, the haematochrome yield of combined extraction technology is 1.42%, slightly below
The haematochrome recovery rate of single extraction（1.60%）, but its colour value is then significantly higher than the haematochrome of single extraction, illustrates present invention connection
Close and extract that the haematochrome purity that obtains is high, quality is good.
Visible with the comparison of comparative example 2 by embodiment, the pectin extraction rate and pectin ester degree of combined extraction technology show
It is higher than single extraction method to write, and illustrates that substituting hydrochloric acid using oxalic acid carries out acidolysis, in combination with ion-exchange, can greatly improve
The recovery rate and quality of pectin.
The foregoing is only presently preferred embodiments of the present invention, all impartial changes done according to scope of the present invention patent with
Modification, should all belong to the covering scope of the present invention.
Claims (1)
1. in a kind of pericarp from dragon fruit combined extracting haematochrome and pectin method, it is characterised in that：Comprise the following steps：
1）By the chopping of fresh dragon fruit pericarp, after 5 ~ 8min of boiling water boiling, clear water rinsing, drying, crushing；
2）By step 1）The gained ethanol that powder adds 5 ~ 10 times of its volume, mass concentration is 70%, extracts 1 ~ 2h, mistake under room temperature
Filter, collects respectively filtrate and filter residue；
3）By step 2）Gained filtrate is concentrated in vacuo to after doing at 50-55 DEG C, is entered with polyethylene glycol/ammonium sulfate double-aqueous phase system
Row abstraction purification；
4）Take step 3）Upper solution, after adding isopyknic chloroform extraction, collects upper strata aqueous phase solution；
5）By step 4）Gained aqueous phase solution is concentrated in vacuo at 50 ~ 55 DEG C, obtains the dragon fruit haematochrome of sticky paste；
6）By step 2）Gained filter residue tap water rinse, adds 5 ~ 10 times of deionized waters of filter residue volume and filter residue weight 1 ~ 3%
Oxalic acid, with sodium hydrate regulator solution pH value be 3.0 ~ 3.6, be then heated to 60 ~ 80 DEG C, slowly stir 60min, filter,
Collect filtrate；
7）By step 6）Gained filtrate adds ion exchange resin, and 30 ~ 60min is slowly stirred under room temperature, filters, and collects filtrate；
8）By step 7）Gained filter vacuum is concentrated into the 1/4 ~ 1/5 of original volume, is subsequently adding the absolute ethyl alcohol of 1-2 times of volume,
Jing centrifugations, precipitation, drying, crushing, obtain final product flaxen jelly powder；
Step 3）Middle polyethylene glycol/ammonium sulfate double-aqueous phase system abstraction purification is specifically by polyglycol solution and ammonium sulfate
In being added to filtrate, Jing after 20 ~ 30min of magnetic agitation, it is 5.0 ~ 5.5 to adjust solution ph, and 6 ~ 12h is stood under room temperature so as to
Layering；
The mass concentration of polyethylene glycol is 15 ~ 25% in the polyethylene glycol/ammonium sulfate double-aqueous phase system, and the quality of ammonium sulfate is dense
Spend for 10 ~ 15%；
Step 7）Described in ion exchange resin be storng-acid cation exchange resin, its consumption for filter residue weight 1 ~ 2%.
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| CN110881594A (en) * | 2019-12-23 | 2020-03-17 | 广西壮族自治区农业科学院 | Preparation method of dragon fruit juice |
| CN110881603A (en) * | 2019-12-24 | 2020-03-17 | 福建农林大学 | Pitaya peel-glucomannan composite microsphere body-shaping solid beverage and preparation method thereof |
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| CN1075729A (en) * | 1992-09-11 | 1993-09-01 | 李有刚 | From orange peel, extract the method for natural yellow pigment, tangerine oil and pectin simultaneously |
| WO2011053106A1 (en) * | 2009-10-30 | 2011-05-05 | Universiti Putra Malaysia | Stabilised colorant composition |
| CN101735648B (en) * | 2010-01-25 | 2013-09-18 | 青岛鹏远康华天然产物有限公司 | Method for separating and purifying beet red pigment by two aqueous phase extraction system |
| CN104211832B (en) * | 2014-09-24 | 2016-08-24 | 广东工业大学 | The preparation method of pectin in dragon fruit pericarp |
| CN104513324A (en) * | 2014-12-17 | 2015-04-15 | 广西壮族自治区农业科学院农产品加工研究所 | Method for extracting pectin from pitaya stem |
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